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- Creators: Barrett, The Honors College

The possibility of creating inorganic/organic hybrid materials has yet to be fully explored within geopolymer research. Using PDMS as an organic precursor, the surface of sodium and potassium geopolymers of varying precursor composition were functionalized with degraded PDMS oligomers. Both types of geopolymer yielded hydrophobic materials with BET surface area of 0.6475 m2/g and 4.342 m2/g for sodium and potassium geopolymer, respectively. Each respective material also had an oil capacity of 74.75 ± 4.06 weight% and 134.19 ± 4.89 weight%. X-ray diffraction analysis demonstrated that the PDMS functionalized sodium geopolymers had similar crystal structures that matched references for zeolite A and sodalite. The potassium geopolymers were amorphous, but showed consistency in diffraction patterns across different compositions.

The following is a report that will evaluate the microstructure of the nickel-based superalloy Hastelloy X and its relationship to mechanical properties in different load conditions. Hastelloy X is of interest to the company AORA because its strength and oxidation resistance at high temperatures is directly applicable to their needs in a hybrid concentrated solar module. The literature review shows that the microstructure will produce different carbides at various temperatures, which can be beneficial to the strength of the alloy. These precipitates are found along the grain boundaries and act as pins that limit dislocation flow, as well as grain boundary sliding, and improve the rupture strength of the material. Over time, harmful precipitates form which counteract the strengthening effect of the carbides and reduce rupture strength, leading to failure. A combination of indentation and microstructure mapping was used in an effort to link local mechanical behavior to microstructure variability. Electron backscatter diffraction (EBSD) and energy dispersive spectroscopy (EDS) were initially used as a means to characterize the microstructure prior to testing. Then, a series of room temperature Vickers hardness tests at 50 and 500 gram-force were used to evaluate the variation in the local response as a function of indentation size. The room temperature study concluded that both the hardness and standard deviation increased at lower loads, which is consistent with the grain size distribution seen in the microstructure scan. The material was then subjected to high temperature spherical indentation. Load-displacement curves were essential in evaluating the decrease in strength of the material with increasing temperature. Through linear regression of the unloading portion of the curve, the plastic deformation was determined and compared at different temperatures as a qualitative method to evaluate local strength.

One of the grand challenges of engineering is to provide access to clean water because it is predicted that by 2025 more than two thirds of the world’s population will face severe water shortages. To combat this global issue, our lab focuses on creating a novel composite membrane to recover potable water from waste. For use as the water-selective component in this membrane design Linde Type A zeolites were synthesized for optimal size without the use of a template. Current template-free synthesis of zeolite LTA produces particles that are too large for our application therefore the particle size was reduced in this study to reduce fouling of the membrane while also investigating the nanoparticle synthesis mechanisms. The time and temperature of the reaction and the aging of the precursor gel were systematically modified and observed to determine the optimal conditions for producing the particles. Scanning electron microscopy, x-ray diffraction, and energy dispersive x-ray analysis were used for characterization. Sub-micron sized particles were synthesized at 2 weeks aging time at -8°C with an average size of 0.6 micrometers, a size suitable for our membrane. There is a limit to the posterity and uniformity of particles produced from modifying the reaction time and temperature. All results follow general crystallization theory. Longer aging produced smaller particles, consistent with nucleation theory. Spinodal decomposition is predicted to affect nucleation clustering during aging due to the temperature scheme. Efforts will be made to shorten the effective aging time and these particles will eventually be incorporated into our mixed matrix osmosis membrane.

This dissertation investigates the potential for stimulating ureolytic and denitrifying microbes concurrently (i.e., stimulating a ureolytic, denitrifying microbial community) for a more efficient microbially induced carbonate precipitation (MICP) process. Three sand columns were run for a treatment period of six weeks with a continuous flow of nutrient solution containing calcium nitrate, calcium acetate, calcium chloride, magnesium sulfate, tryptic soy broth and trace metals. The first and third columns served as control columns, within which only denitrification processes were at work. The first column was used for periodic sampling to measure the pH, ion concentrations, and total nitrogen over time. The third column was used to measure compressional (P-) and shear (S-) wave velocities to monitor cementation and desaturation over time. The second column was subject to initial conditions identical to the other two columns except that urea was added to the nutrient solution to stimulate ureolysis and was also subject to sampling. This was done to determine whether the use of the combined MICP processes resulted in increased efficiency of precipitation. Results from ion chromatography analysis, acid digestion and scanning electron microscope imaging did not show an increase in the amount of carbonate precipitated for the second column, possibly due to nitrite inhibition and abiotic hydrolysis of the urea from sterilization of the nutrient solution through autoclaving. However, the stimulation of denitrification and ureolysis in combination was achieved, and the amount of carbonate precipitation per mol of nitrate reduced increased, which in a sense increased the efficiency of the system. Ultimately, more experimentation is needed to determine if this combination is beneficial for MICP.
The study of the mechanical behavior of nanocrystalline metals using microelectromechanical systems (MEMS) devices lies at the intersection of nanotechnology, mechanical engineering and material science. The extremely small grains that make up nanocrystalline metals lead to higher strength but lower ductility as compared to bulk metals. Effects of strain-rate dependence on the mechanical behavior of nanocrystalline metals are explored. Knowing the strain rate dependence of mechanical properties would enable optimization of material selection for different applications and lead to lighter structural components and enhanced sustainability.

The goal of this research is to compare the mechanical properties of CP-Ti and Ti-O and to understand the relationship between a material's microstructure and its response to fatigue. Titanium has been selected due to its desirable properties and applicability in several engineering fields. Both samples are polished and etched in order to visualize and characterize the microstructure and its features. The samples then undergo strain-controlled fatigue tests for several thousand cycles. Throughout testing, images of the samples are taken at zero and maximum load for DIC analysis. The DIC results can be used to study the local strains of the samples. The DIC analysis performed on the CP-Ti sample and presented in this study will be used to understand how the addition of oxygen in the Ti-O impacts fatigue response. The outcome of this research can be used to develop long-lasting, high strength materials.

A model has been developed to modify Euler-Bernoulli beam theory for wooden beams, using visible properties of wood knot-defects. Treating knots in a beam as a system of two ellipses that change the local bending stiffness has been shown to improve the fit of a theoretical beam displacement function to edge-line deflection data extracted from digital imagery of experimentally loaded beams. In addition, an Ellipse Logistic Model (ELM) has been proposed, using L1-regularized logistic regression, to predict the impact of a knot on the displacement of a beam. By classifying a knot as severely positive or negative, vs. mildly positive or negative, ELM can classify knots that lead to large changes to beam deflection, while not over-emphasizing knots that may not be a problem. Using ELM with a regression-fit Young's Modulus on three-point bending of Douglass Fir, it is possible estimate the effects a knot will have on the shape of the resulting displacement curve.

Although wind turbine bearings are designed to operate 18-20 years, in the recent years premature failure among these bearings has caused this life to reduce to as low as a few months to a year. One of the leading causes of premature failure called white structure flaking is a mechanism that was first cited in literature decades ago but not much is understood about it even today. The cause of this mode of failure results from the initiation of white etched cracks (WECs). In this report, different failure mechanisms, especially premature failure mechanisms that were tested and analyzed are demonstrated as a pathway to understanding this phenomenon. Through the use of various tribometers, samples were tested in diverse and extreme conditions in order to study the effect of these different operational conditions on the specimen. Analysis of the tested samples allowed for a comparison of the microstructure alterations in the tested samples to the field bearings affected by WSF.

The transition to lead-free solder in the electronics industry has benefited the environment in many ways. However, with new materials systems comes new materials issues. During the processing of copper pads, a protective surface treatment is needed to prevent the copper from oxidizing. Characterizing the copper oxidation underneath the surface treatment is challenging but necessary for product reliability and failure analysis. Currently, FIB-SEM, which is time-consuming and expensive, is what is used to understand and analyze the surface treatment-copper oxide(s)-copper system. This project's goals were to determine a characterization methodology that cuts both characterization time and cost in half for characterizing copper oxidation beneath a surface treatment and to determine which protective surface treatment is the best as defined by multiple criterion such as cost, sustainability, and reliability. Two protective surface treatments, organic solderability preservative (OSP) and chromium zincate, were investigated, and multiple characterization techniques were researched. Six techniques were tested, and three were deemed promising. Through our studies, it was determined that the best surface treatment was organic solderability preservative (OSP) and the ideal characterization methodology would be using FIB-SEM to calibrate a QCM model, along with using SERA to confirm the QCM model results. The methodology we propose would result in a 91% reduction in characterization cost and a 92% reduction in characterization time. Future work includes further calibration of the QCM model using more FIB/SEM data points and eventually creating a model for oxide layer thickness as a function of exposure time and processing temperature using QCM as the primary data source. An additional short essay on the role of SEM on the continuing miniaturization of integrated circuits is included at the end. This paper explores the intertwined histories of the scanning electron microscope and the integrated circuit, highlighting how advances in SEM influence integrated circuit advances.

The story of graphene truly began in what was simply a stub in the journal Physical Review not two years after the end of World War II. In 1947, McGill University physicist P.R. Wallace authored “The Band Theory of Graphite” and attempted to develop a foundation on which the structure-property relationship of graphite could be explored; he calculates the number of free electrons and conductivity of what he describes as “a single hexagonal layer” and “suppos[es] that conduction takes place only in layers” in bulk graphite to predict wave functions, energies at specific atomic sites in the hexagonal lattice, and energy contours using a tight binding approximation for a hypothesized version of what we now call ‘armchair-style’ graphene. While Wallace was the first to explore the band structure and Brillouin Zones of single-layer graphite, the concept of two-dimensional materials was not new. In fact, for years, it was dismissed as a thermodynamic impossibility.
Everything seemed poised against any proposed physical and experimental stability of a structure like graphene. “Thermodynamically impossible”– a not uncommon shutdown to proposed novel physical or chemical concepts– was once used to describe the entire field of proposed two-dimensional crystals functioning separately from a three-dimensional base or crystalline structure. Rudolf Peierls and Lev Davoidovich Landau, both very accomplished physicists respectively known for the Manhattan Project and for developing a mathematical theory of helium superfluidity, rejected the possibility of isolated monolayer to few-layered crystal lattices. Their reasoning was that diverging thermodynamic-based crystal lattice fluctuations would render the material unstable regardless of controlled temperature. This logic is flawed, but not necessarily inaccurate– diamond, for instance, is thermodynamically metastable at room temperature and pressure in that there exists a slow (i.e. slow on the scale of millions of years) but continuous transformation to graphite. However, this logic was used to support an explanation of thermodynamic impossibility that was provided for graphene’s lack of isolation as late as 1979 by Cornell solid-state physicist Nathaniel David Mermin. These physicists’ claims had clear and consistent grounding in experimental data: as thin films become thinner, there exists a trend of a decreasing melting temperature and increasing instability that renders the films into islands at somewhere around ten to twenty atomic layers. This is driven by the thermodynamically-favorable minimization of surface energy.